H.-L. Zhu

Crystal structure of 1,2-diaminopropanesilver(I) 4-nitrobenzoate dihydrate, Ag(C3H6N2H6)(C7H3NO4) · 2H2O

Abstract C10H18AgN3O6, triclinic, P1 (No. 2), a = 7.139(2) Å, b = 7.509(2) Å, c = 14.007(4) Å, α = 78.505(5)°, β = 78.789(4)°, γ = 82.023(4)°, V = 717.8 Å3, Z = 2, Rgt(F) = 0.036, wRref(F2) = 0.096, T = 298 K.

Crystal structure of 1,2-diaminopropanesilver(I) 3,5-dinitrobenzoate - ammonia (1 :1), Ag(C3H10N2)(C7H3N2O6) . NH3

Discussion Coordination compounds of the coinage monovalent ions have received considerable attention in the last thirty years. In particular, the study of their biological activity is of importance. Silver is by far the less investigated coinage metal in coordination chemistry, which possibly be attributed to the poor solubility of silver® compounds in common solvents and the sensitivity toward photode composition [ 1 ]. On the other hand, it has been found that many factors such as the nature of the ligands, solvents, counter-anions, etc., appear to modulate the stereochemistry of silver complexes. Our previous studies on the coordination of various silver® salts to a macrocyclic Schiff base have clearly shown the versatility [2,3]. As a continuation of these studies, we have synthesized and characterized silver(I)carboxylic complex of 1,2-diaminopropane, which is a single-brand helical complex. The title complex crystallizes with two crystallographically equivalent [Ag(pren)](dnbc)(NH3) symmetric units per unit cell (where pren is 1,2-diaminopropane and dnbc is 3,5-dinitrobenzoate anion), and one crystal lattice ammonia molecule. There is one silver(I) atom in each symmetric unit, which is two coordinated to two nitrogen atoms from different pren ligands. The average silver-nitrogen bond length (2.151(5) Â) is in the normal distance of Ag—Ν (primary amine). The N-Ag-N angle of 163.5(2)° is significantly deviated from 180°, indicating a larger geometry strain around silver atom. All pren molecules in the complex are in ira«s-conformation, which join the silver atoms along α-axis to form a one-dimensional helical chain. All the oxygen atoms from the ligand groups in the title complex do not participate in coordinating, but some of them contribute to the fo rma t ion of a great deal of weak in te rac t ions . The non-coordinated molecular NH3 join the neighboring silver atoms (d(N—Ag) = 3.240(5) Â and 2.955(5) Â), forming a double single-helical chain. Abstract CioHieAgNsOe, tricMc, PI (No. 2), a = 5.640(5)Á, b = 9.499(8)Â, c = 14.84(2) Á, a = 84.24(1)°, β = 79.05(2)°, γ = 72.731(8)°, V= 744.8 À, Z = 2, Rgí(F) = 0.044, wRk/f) = 0.111, T= 298 K.

Crystal structure of ethylenediaminesilver(I) 4-nitrobenzoate hemi-hydrate, Ag(C2H8N2)(C7H4No4) · 0.5H2O

C9Hi3AgN3O4.50, monoclinic, C12/cl (No. 15), a = 8.331(2) Â, ¿=11.645(2) Â, c = 23.947(5) Â, β = 94.845(3)°, V = 2314.8 Á, Ζ = 8, Rgt(F) = 0.030, wRlef(F) = 0.072, Τ = 298 Κ. Source of material Ag:0 (0.5 mmol, 116 mg) and 4-nitrobenzoate (1 mmol, 167 mg) were dissolved in a 1 : 1 solution of acetonitrile and concentrated ammonium solution (v/v, 10 ml), stirring for ca. 10 min ethylenediamine (1 mmol, 60 mg) was added to obtain a clear solution. After standing still the solution in air for two days with the ammium gas escaping large colorless prism crystals were crystallized, isolated, washed with water for three times, and dried in a vacuum desiccator under drying CaCh (yield 45%). Elemental analysis: found C, 31.70%; H, 3.90%; N, 12.14%; calc. for C9Hi3AgN304.5 C, 31.51%; H, 3.82%; N, 12.25%. Discussion Coordination chemistry of coinage metal(I) monovalent ions have received considerable attention in the past three decades. The research on different uses and ideas of various silver® compounds is being in the ascendant. We have been interested in the investigation on silver® complexes with various organic ligands containing Ν and/or O atoms. Reported here is a silr(I)carboxylato complex with ethylenediamine. The title complex crystallizes with the asymmetric unit consisting °f one Ag ions, one 4-nitrobenzoate anion, one ethylenediamine molecule, and half a crystal water molecule. The Ag(l) ion is coAg(1A) ordinated by two nitrogen atoms from two ethylenediamines. The Ag—Ν distances are 2.138(3) Á and 2.148(3) À and the N-Ag-N angle is 173.1(2)°, indicating a linear coordination of Ag(l). Besides, there is a ligand unsupported Ag—Ag bond with a <i(Ag---Ag) distance of2.934(3) A. The nitrobenzoate anion is pendent and functions as a counterion to maintain charge balance. The amine ligands bridge adjacent Ag ions to form one-dimensional chain and the chains are linked by Ag—Ag bonds to form two-dimensional layer with (4,4) topology. The four-connected nodes are provided by pairs of Ag ions. In addition, there are a variety of hydrogen bonds N H O , O H O and C H 0 [d(Nl-03) = 3.070(3) Á; ¿ (N1-04) = 2.968(4) À; d(N2-05) = 3.060(2) Á; d(N2-04) = 3.022(4) A; d(05 03) = 2.803(1) Â, ¿ (C3-02) = 2.714(0) À; d(C4-04) = 2.784(7) Â; d(C7-01) = 2.726(8) Â] which extend the two-dimensional layer into three-dimensional supramolecular auay. Table 1. Data collection and handling. Crystal: colorless prism, size 0.20 χ 0.30 χ 0.30 mm Wavelength: Mo Ka radiation (0.71073 A) μ: 17.55 cnT Diffractometer, scan mode: Bruker SMART CCD. φ/ω 20max: 52.72° N(hkl) measured, N(hkl)amqus: 6470, 2309 Criterion for 10bs, N(hkl)gc. 7obs>2ff(/obs), 1862 N(param) refined: 211 Programs: SHELXTL [1], SHELXTL-plus [2] Correspondence author (e-mail: hlzhu@wist.edu.cn) 244 Ag(C2H8N2)(C7H4N04) · 0 .5Η ? 0 Table 2. Atomic coordinates and displacement parameters (in Â). Atom Site X y ζ Ui so H(l) 8/ 0.334(5) 0.016(3) 0.572(2) 0.05(1) H(2) 8/ 0.287(4) 0.135(3) 0.649(2) 0.039(9) H(3) 8/ -0.020(4) 0.320(3) 0.552(1) 0.040(9) H(4) 8/ 0.020(5) 0.194(3) 0.479(2) 0.06(1) H(5) 8/ 1.230(4) -0.104(3) 0.669(2) 0.04(1) H(6) 8/ 1.207(4) -0.143(3) 0.724(2) 0.040(9) H(7) 8/ 0.739(6) 0.102(4) 0.728(2) 0.08(2) Table 2. Continued. Atom Site X y ζ U, s„ H(8) 8/ 0.836(4) 0.186(3) 0.719(2) 0.05(1) H(9) 8/ 1.008(4) -0.256(3) 0.684(1) 0.035(9) H(10) 8/ 1.011(4) -0.219(2) 0.625(2) 0.037(9) H( l l ) 8/ 0.642(4) 0.129(3) 0.634(1) 0.033(9) H(12) 8/ 0.771(3) 0.210(2) 0.628(1) 0.023(8) H(13) 8/ 0.000(6) 0.492(3) 0.725(2) 0.05(1) Table 3. Atomic coordinates and displacement parameters (in À). Atom Site X y ζ U H U22 C/33 U12 U13 t/23 Ag(l) 8/ 0.97424(3) 0.00715(2) 0.68864(1) 0.0430(2) 0.0342(2) 0.0402(2) 0.0154(1) -0.0026(1) -0.0033(1) N(l) 8/ 1.1547(3) -0.1241(2) 0.6862(1) 0.032(2) 0.030(1) 0.037(2) 0.006(1) 0.000(1) -0.001(1) N(2) 8/ 0.7937(4) 0.1327(3) 0.7014(1) 0.039(2) 0.030(1) 0.038(2) 0.010(1) -0.004(1) -0.003(1) N(3) 8/ 0.1047(4) 0.3182(3) 0.6592(1) 0.054(2) 0.055(2) 0.045(2) -0.007(2) 0.008(2) 0.001(2) 0(1) 8/ 0.1338(4) 0.0425(2) 0.4281(1) 0.086(2) 0.060(2) 0.035(2) 0.009(2) -0.001(1) -0.010(1) 0(2) 8/ 0.3045(4) -0.0546(3) 0.4803(1) 0.091(2) 0.084(2) 0.055(2) 0.037(2) -0.008(2) -0.020(2) 0(3) 8/ 0.0006(3) 0.3947(2) 0.6519(1) 0.045(1) 0.048(1) 0.046(2) 0.015(1) -0.000(1) -0.007(1) 0(4) 8/ 0.1955(3) 0.3020(2) 0.7027(1) 0.073(2) 0.066(2) 0.032(2) 0.020(1) -0.016(1) -0.011(1) 0(5) 4e 0 0.5259(4) 3/4 0.068(3) 0.040(2) 0.049(3) 0 0.015(2) 0 C(l) 8/ 0.2074(4) 0.0237(2) 0.4732(1) 0.038(2) 0.030(2) 0.027(2) -0.000(1) -0.000(1) -0.004(1) C(2) 8/ 0.1769(4) 0.0964(3) 0.5209(1) 0.036(2) 0.037(2) 0.031(2) -0.003(1) 0.003(1) -0.002(1) C(3) 8/ 0.2584(4) 0.0736(3) 0.5722(1) 0.037(2) 0.034(2) 0.037(2) 0.003(1) -0.000(1) 0.001(1) C(4) 8/ 0.2311(4) 0.1445(3) 0.6171(2) 0.035(2) 0.035(2) 0.032(2) -0.003(1) -0.004(1) 0.003(1) C(5) 8/ 0.1270(3) 0.2376(2) 0.6103(1) 0.030(2) 0.032(2) 0.029(2) -0.006(1) 0.003(1) 0.001(1) C(6) 8/ 0.0454(4) 0.2569(3) 0.5578(1) 0.039(2) 0.038(2) 0.037(2) 0.009(2) 0.001(2) 0.004(1) C(7) 8/ 0.0692(4) 0.1859(3) 0.5134(1) 0.043(2) 0.046(2) 0.026(2) 0.001(2) -0.003(1) 0.004(2) C(8) 8/ 1.0820(4) -0.2317(3) 0.6631(2) 0.029(2) 0.034(2) 0.042(2) 0.002(1) -0.004(2) -0.000(1) C(9) 8/ 0.7014(4) 0.1768(3) 0.6509(2) 0.036(2) 0.030(2) 0.037(2) 0.002(1) -0.002(2) -0.004(1) Acknowledgment. The authors thank the Education Office of Hubei Province for the research grant 2002B29002.

Crystal structure of 4-aminobenzenesulfonosilver(I), C6H6AgNO3S

Abstract C6H6AgNO3S, monoclinic, P121/c1 (No. 14), a = 9.109(5) Å, b = 8.910(5) Å, c = 9.546(6) Å, β = 100.076(7)°, V = 762.8 Å3, Z = 4, Rgt(F) = 0.030, wRref(F2) = 0.078, T = 293 K.

Crystal structure of ethylenediammonium di(4-chlor-benzoate), (C2H10N2)(C7H4O2Cl)2

Abstract C16H18Cl2N2O4, monoclinic, C12/c1 (No. 15), a = 21.92(1) Å, b = 9.015(5) Å, c = 8.620(5) Å, β = 96.151(9)°, V = 1693.3 Å3, Z = 4, Rgt(F) = 0.064, wRref(F2) = 0.186, T = 298 K.

Crystal structure of ethylenediaminesilver(I) di(3,5-dinitrobenzoato)- silver(I) dihydrate, Ag2(C2H8N2)(C7H3N2O6)2 · 2H2O

Abstract C16H18Ag2N6O14, triclinic, P1̅ (No. 2), a = 6.978(2) Å, b = 12.919(5) Å, c = 15.029(5) Å, α = 84.320(6)°, β = 76.81 (5)°, ϒ = 79.612(6)°, V = 1295.1 Å3, Z = 2, Rgt(F) = 0.065, wRref(F2) = 0.091, T = 298 K.

Crystal structure of 1,2-ethylenediaminesilver(I) bis(4-nitrobenzoato)-silver(I), C16H16Ag2N4O8

Abstract C16H16Ag2N4O8, triclinic, P1̅ (No. 2), a = 6.346(3) Å, b = 7.022(3) Å, c = 23.04(1) Å, α = 82.638(7)°, β = 83.169(6)°, ϒ = 67.880(6)°, V = 940.6 Å3, Z = 2, Rgt(F) = 0.031, wRref(F2) = 0.070, T = 298 K.

Crystal structure of aqua-bis(4-nitrobenzoato)disilver(I), Ag2(C7H4NO4)2(H2O)

Abstract C14H10Ag2N2O9, monoclinic, C12/c1 (No. 15), a = 21.164(6) Å, b = 6.451(2) Å, c = 12.219(4) Å, β = 104.646(4)°, V = 1614.1 Å3, Z = 4, Rgt(F) = 0.035, wRref(F2) = 0.074, T = 298 K.

Crystal structure of 1,2-diaminopropanesilver(I) 3,5-dinitrobenzoate hydrate, Ag(C3H10N2)(C7H3N2O6) · 1.5H2O

Abstract C10H16AgN4O7.50, monoclinic, C12/c1 (No. 15), a = 28.123(8) Å, b = 5.241(2) Å, c = 24.723(7) Å, β = 122.958(4)°, V = 3057.9Å3, Z = 8, Rgt(F) = 0.037, wRref(F2) = 0.070, T = 298 K.